CN114932376A - Batch heat treatment device for hollow fiber electrodes, manufacturing method and application - Google Patents

Batch heat treatment device for hollow fiber electrodes, manufacturing method and application Download PDF

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Publication number
CN114932376A
CN114932376A CN202210494162.XA CN202210494162A CN114932376A CN 114932376 A CN114932376 A CN 114932376A CN 202210494162 A CN202210494162 A CN 202210494162A CN 114932376 A CN114932376 A CN 114932376A
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heat treatment
hollow fiber
fiber electrode
box body
batch
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CN114932376B (en
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陈为
吴钢锋
董笑
陈奥辉
宋艳芳
李桂花
魏伟
孙予罕
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Shanghai Advanced Research Institute of CAS
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Shanghai Advanced Research Institute of CAS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23PMETAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
    • B23P15/00Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0068Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention provides a batch heat treatment device for hollow fiber electrodes, a manufacturing method and application, wherein the manufacturing method comprises the following steps: s1, mechanically cutting and bending the raw materials into a box body, and welding and forming; s2, fixing the box body at the periphery; and S3, arranging a plurality of partition layers in the box body, and then placing the box body in a tubular furnace for roasting treatment to obtain the heat treatment device. The hollow fiber electrode batch heat treatment device manufactured by the manufacturing method is applied to batch heat treatment of the hollow fiber electrode. The invention provides a device which is simple in design, simple and convenient to operate and capable of being used for batch heat treatment of hollow fiber electrodes quickly and efficiently.

Description

Batch heat treatment device for hollow fiber electrodes, manufacturing method and application
Technical Field
The invention belongs to the technical field of chemical engineering and processes, and particularly relates to a batch heat treatment device for hollow fiber electrodes, a manufacturing method and application.
Background
The ever-increasing total energy demand and over-exploitation of fossil fuels leads to global CO 2 The total emissions continue to rise, causing increasingly serious environmental problems. The electrochemical conversion synthetic chemical driven by renewable electric energy is developed by combining with the development and utilization of rapidly developed renewable energy, and the electrochemical conversion synthetic chemical has important significance for improving the energy structure and driving the sustainable development of the economy and the society and upgrading the industry.
Compared with the traditional electrode catalyst prepared by the conductive agent and the adhesive, the self-supporting hollow fiber electrode has good conductivity and catalytic activity, the unique structure of the self-supporting hollow fiber electrode can be used as an ideal place for the reaction of gas and liquid raw materials, the contact of a reaction medium is fully promoted, and the diffusion and the migration of reactants and products are facilitated. Meanwhile, the material has good mechanical strength and stability, can maintain stable structure and performance in a long-period test, and shows huge industrial application potential. However, due to the high aspect ratio of the hollow fiber electrode, the efficiency of large-scale heat treatment and the yield of products are not ideal. Therefore, the system capable of rapidly and efficiently carrying out batch heat treatment on the hollow fiber electrode is designed, so that the production efficiency is improved, the uniformity and repeatability of the electrode material are ensured, and the industrial application prospect of the system is further improved.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a batch heat treatment apparatus for hollow fiber electrodes, a manufacturing method and an application thereof, which are used to solve the problems of low production efficiency and incapability of ensuring uniformity and repeatability of electrode materials due to the inability of efficient batch heat treatment of hollow fiber electrodes in the prior art.
To achieve the above and other related objects, the present invention provides a method for manufacturing a batch heat treatment apparatus for hollow fiber electrodes, the method comprising the steps of:
s1, mechanically cutting and bending the raw materials into a box body, and welding and forming;
s2, fixing the box body at the periphery;
and S3, arranging a plurality of partition layers in the box body, and then placing the box body in a tubular furnace for roasting treatment to obtain the heat treatment device.
Preferably, the raw material in step S1 is one or a combination of a titanium plate, a titanium mesh, a tungsten plate and a tungsten mesh.
Preferably, the thickness of the raw material in step S1 is 0.1-2.5 mm.
Preferably, the shape of the case in step S1 is one of a rectangular parallelepiped, a cylinder, a semi-cylinder, a 3/4 cylinder, and a 2/3 cylinder.
Preferably, the welding method in step S1 is one or a combination of shielded metal arc welding, argon arc welding and laser welding.
Preferably, the fixing manner in step S2 is one of titanium bar constraint fixing, tungsten bar constraint fixing and mechanical casting fixing.
Preferably, the distance between two adjacent partition layers in the step S3 is 5-10 mm.
Preferably, the shape of the partition layer in step S3 is one or a combination of zigzag, corrugated, and honeycomb shapes.
Preferably, the arrangement direction of the partition layer in step S3 is one or more of a transverse partition, a longitudinal partition and an oblique partition.
Preferably, the roasting atmosphere in the step S3 is an oxygen or air atmosphere, and the roasting atmosphere flow rate is 100 to 300 mL/min.
Preferably, in the step S3, the heating rate of the roasting is 1-20 ℃/min, the roasting temperature is 400-1000 ℃, and the roasting time is 4-12 h.
The present invention also provides a hollow fiber electrode batch heat treatment apparatus manufactured by the manufacturing method of the hollow fiber electrode batch heat treatment apparatus, the heat treatment apparatus including:
the box body is in a cuboid, cylinder, semi-cylinder, 3/4 cylinder or 2/3 cylinder shape, and an anti-deformation structure is fixed along the length direction of the box body;
the partition layer, it is provided with a plurality ofly to block the layer, and is a plurality of block the even setting in of layer in inside the box, just block the layer and be zigzag, corrugated or honeycombed.
The invention also provides application of the hollow fiber electrode batch heat treatment device, and the hollow fiber electrode batch heat treatment device is applied to batch heat treatment of the hollow fiber electrode, and specifically comprises the following steps:
a1, providing the hollow fiber electrode batch heat treatment device;
a2, sequentially placing hollow fiber electrode blanks pre-filled in a liner tube into the partition layer of the heat treatment device in batches;
a3, placing the heat treatment device provided with the hollow fiber electrode blank in a tube furnace, carrying out first heat treatment in an air atmosphere, and then carrying out second heat treatment in a gas atmosphere to obtain a batch of hollow fiber electrodes.
Preferably, the hollow fiber electrode blank in the step a2 is made of one of silver, copper, iron, cobalt, nickel, titanium, bismuth oxide and tin oxide;
the length of the hollow fiber electrode blank is 100-200 mm.
Preferably, the atmosphere of the first heat treatment in the step a3 is air; the flow rate of the atmosphere for the first heat treatment is 100-200 mL/min; the temperature rise rate of the first heat treatment is 1-5 ℃/min; the temperature of the first heat treatment is 550-600 ℃; the time of the first heat treatment is 4-6 h.
Preferably, the atmosphere of the second heat treatment in the step a3 is one of hydrogen, argon and hydrogen/argon mixture; the flow rate of the atmosphere for the second heat treatment is 50-1000 mL/min; the temperature rise rate of the second heat treatment is 1-20 ℃/min, the temperature of the second heat treatment is 100-1600 ℃, and the time of the second heat treatment is 0.5-24 h.
As described above, the batch heat treatment apparatus for hollow fiber electrodes, the manufacturing method and the application of the invention have the following advantages:
the invention provides a device which is simple in design, simple and convenient to operate and capable of being used for batch heat treatment of hollow fiber electrodes quickly and efficiently, metal titanium or tungsten with high melting point, low mass density, strong bending ductility, strong corrosion resistance and strong oxidation resistance is used as a raw material of the device, the device is fixedly formed by mechanical cutting and bending welding, and partition layers with different structural forms are arranged in the device, so that the device can be ensured to be stable under high-temperature oxidation or reduction conditions, and cannot pollute a target material, the uniformity of a thermal radiation field and a gas flow field in the heat treatment process is controlled, the uniformity and repeatability of heat treatment of the target material are ensured, the target material can be subjected to heat treatment quickly and massively, and the production efficiency is greatly improved.
The batch heat treatment device can be used for batch treatment of hundreds to thousands of hollow fiber electrode samples once, effectively simplifies the batch production process of the hollow fiber electrodes, improves the production efficiency, forms an efficient, stable and low-cost preparation process amplification scheme, promotes large-scale production and application of the hollow fiber electrodes, can be widely applied to the production process of various hollow fiber electrodes, and has extremely high application prospects.
Drawings
FIG. 1 is a front view showing a batch heat treatment apparatus for hollow fiber electrodes in embodiment 5 of the present invention.
FIG. 2 is a left side view showing a batch heat treatment apparatus for hollow fiber electrodes in example 5 of the present invention.
Description of the element reference numerals
10. A box body; 20. and a partition layer.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Please refer to fig. 1-2. It should be noted that the drawings provided in this embodiment are only for schematically illustrating the basic idea of the present invention, and the components related to the present invention are only shown in the drawings and not drawn according to the number, shape and size of the components in actual implementation, and the form, quantity and proportion of each component in actual implementation may be arbitrarily changed, and the component layout may be more complicated.
The invention provides a device which is simple in design, simple and convenient to operate and capable of being used for batch heat treatment of hollow fiber electrodes quickly and efficiently, metal titanium or tungsten with high melting point, low mass density, strong bending ductility, strong corrosion resistance and strong oxidation resistance is used as raw materials of the device, the device is fixedly formed by mechanical cutting and bending welding, and partition layers with different structural forms are arranged in the device, so that the device can be ensured to be stable under high-temperature oxidation or reduction conditions without polluting a target material, the uniformity of a thermal radiation field and a gas flow field in the heat treatment process is controlled, the uniformity and repeatability of heat treatment of the target material are ensured, the target material can be subjected to heat treatment quickly and in large batch, and the production efficiency is greatly improved; the batch heat treatment device can be used for batch treatment of hundreds to thousands of hollow fiber electrode samples in a single time, effectively simplifies the batch production process of the hollow fiber electrodes, improves the production efficiency, forms an efficient, stable and low-cost preparation process amplification scheme, promotes the large-scale production and application of the hollow fiber electrodes, can be widely applied to the production process of various hollow fiber electrodes, and has extremely high application prospect.
The invention provides a manufacturing method of a batch heat treatment device for hollow fiber electrodes, which comprises the following steps:
s1, mechanically cutting and bending the raw materials into a box body 10, and welding and forming;
s2, fixing the box body 10 at the periphery;
s3, disposing a plurality of barrier layers 20 inside the case 10, and then placing the case in a tube furnace to perform a baking process to obtain a heat treatment apparatus.
As an example, the raw material in step S1 is one or a combination of a titanium plate, a titanium mesh, a tungsten plate, and a tungsten mesh.
Specifically, the titanium or tungsten has high melting point, strong corrosion resistance and strong oxidation resistance, and when the titanium or tungsten is used as a raw material of the box body 10, the titanium or tungsten can be used for carrying out heat treatment on the hollow fiber electrode sample without influencing the electrode material in oxidation or reduction; preferably, the raw material is a titanium mesh having a pore size of 2 x 4 mm.
As an example, the thickness of the raw material in step S1 is 0.1-2.5 mm, such as 0.1mm, 0.5mm, 1.0mm, 1.5mm, 2.0mm, 2.5mm, etc.
Preferably, the thickness of the raw material is 1.0-1.5 mm, such as 1.0mm, 1.1mm, 1.2mm, 1.3mm, 1.4mm, 1.5mm, etc.
As an example, the length of the raw material in step S1 is 400-700 mm, such as 400mm, 500mm, 600mm, 700mm, etc.
Specifically, the length of the raw material used is determined according to the length of the hollow fiber electrode blank to be actually processed, and is not limited herein, and preferably, the length of the raw material is 500 to 650mm, such as 500mm, 550mm, 600mm, 650mm, and the like.
As an example, the shape of the case 10 in step S1 is one of a rectangular parallelepiped, a cylinder, a semi-cylinder, a 3/4 cylinder, and a 2/3 cylinder.
The housing 10 is preferably shaped as an 3/4 cylinder, as shown with reference to fig. 1 and 2.
As an example, the welding method in step S1 is one or a combination of shielded metal arc welding, argon arc welding and laser welding.
Preferably, the welding method is argon arc welding.
As an example, the fixing manner in step S2 is one of titanium rod constraint fixing, tungsten rod constraint fixing, and mechanical cast-pressing fixing.
Specifically, the titanium rod constraint and fixation or the tungsten rod constraint and fixation is to wind the titanium rod or the tungsten rod around the box body 10; preferably, the fixing mode is that the titanium rod is restrained and fixed; more preferably, the titanium rod used for constraint fixing is in the shape of a circular arc.
By way of example, the distance between two adjacent partition layers 20 in step S3 is 5-10 mm, such as 5mm, 6mm, 7mm, 8mm, 9mm, 10mm, etc.
Preferably, the distance between two adjacent partition layers 20 is 6-8 mm, such as 6mm, 6.5mm, 7mm, 7.5mm, 8mm, etc.
As an example, the shape of the partition layer 20 in step S3 is one of or a combination of a zigzag shape, a wave shape, and a honeycomb shape.
Preferably, the partition layer 20 has a honeycomb shape.
As an example, the arrangement direction of the partition layer 20 in step S3 is one or more of a lateral partition, a longitudinal partition, and an oblique partition.
Specifically, the arrangement of the partition layer 20 can improve the uniformity of the heated material and the sufficiency of the contact with the air flow in the heat treatment process, and meanwhile, the arrangement of the partition layer 20 can divide the internal space of the box body 10 into a plurality of independent spaces, so that the heat treatment operation can be performed quickly and in large batch; preferably, the partition layer 20 is disposed in a direction of a lateral partition.
For example, the atmosphere for calcination in step S3 is an oxygen or air atmosphere, and the flow rate of the atmosphere for calcination is 100 to 300mL/min, such as 100mL/min, 150mL/min, 200mL/min, 250mL/min, 300mL/min, and the like.
Preferably, the flow rate of the roasting atmosphere is 100-200 mL/min, such as 100mL/min, 120mL/min, 140mL/min, 160mL/min, 180mL/min, 200mL/min, and the like.
For example, in step S3, the temperature increase rate of the baking is 1 to 20 ℃/min, such as 1 ℃/min, 2 ℃/min, 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min, etc., the baking temperature is 400 to 1000 ℃, such as 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃, etc., and the baking time is 4 to 12 hours, such as 4 hours, 6 hours, 8 hours, 10 hours, 12 hours, etc.
Specifically, a compact oxide layer is generated on the surface of the raw material through high-temperature roasting; preferably, the heating rate of the roasting is 1-10 ℃/min, such as 1 ℃/min, 3 ℃/min, 5 ℃/min, 7 ℃/min, 9 ℃/min, 10 ℃/min and the like, the roasting temperature is 600-800 ℃, such as 600 ℃, 650 ℃, 700 ℃, 750 ℃, 800 ℃ and the like, and the roasting time is 6-8 h, such as 6h, 6.5h, 7h, 7.5h, 8h and the like.
The invention also provides a batch heat treatment device for the hollow fiber electrode, which is manufactured by the manufacturing method and comprises the following steps: the box body 10 is a cuboid, a cylinder, a semi-cylinder, an 3/4 cylinder and a 2/3 cylinder, and an anti-deformation structure is fixed along the length direction of the box body 10; the partition layer 20 is provided with a plurality ofly, and a plurality of partition layers 20 are even sets up inside box 10, and partition layer 20 is zigzag, corrugated or honeycomb.
In order to better understand the batch heat treatment device and the manufacturing method of the hollow fiber electrode in the invention, the invention also provides an application of the batch heat treatment device of the hollow fiber electrode, and the batch heat treatment device of the hollow fiber electrode is applied to the batch heat treatment of the hollow fiber electrode, and specifically comprises the following steps:
a1, providing the hollow fiber electrode batch heat treatment device;
a2, sequentially putting the hollow fiber electrode blanks pre-filled in the liner tube into the partition layer 20 of the heat treatment device in batches;
a3, placing the heat treatment device with the hollow fiber electrode blank in a tube furnace, carrying out first heat treatment in an air atmosphere, and then carrying out second heat treatment in a gas atmosphere to obtain a batch of hollow fiber electrodes.
For example, the material of the hollow fiber electrode blank in step a2 is one of silver, copper, iron, cobalt, nickel, titanium, bismuth oxide, and tin oxide; the length of the hollow fiber electrode blank is 100-200 mm, such as 100mm, 120mm, 140mm, 160mm, 180mm, 200mm and the like; preferably, the length of the hollow fiber electrode green body is 160mm, 180 mm.
Specifically, the hollow fiber electrode soft body is straightened, dried, kept stand and cut to obtain a cut hollow fiber electrode blank, the hollow fiber electrode blank is filled into a corresponding liner tube for subsequent heat treatment, and in the invention, the hollow fiber electrode blank which is pre-filled in the liner tube is placed in a heat treatment device for heat treatment.
As an example, the atmosphere of the first heat treatment in step a3 is air; the flow rate of the atmosphere for the first heat treatment is 100-200 mL/min, such as 100mL/min, 120mL/min, 140mL/min, 160mL/min, 180mL/min, 200mL/min, and the like; the temperature rise rate of the first heat treatment is 1-5 ℃/min, such as 1 ℃/min, 2 ℃/min, 3 ℃/min, 4 ℃/min, 5 ℃/min and the like; the temperature of the first heat treatment is 550-600 ℃, such as 550 ℃, 560 ℃, 570 ℃, 580 ℃, 590 ℃, 600 ℃ and the like; the time of the first heat treatment is 4-6 h, such as 4h, 4.5h, 5h, 5.5h, 6h and the like.
Specifically, the first heat treatment is an oxidation process in air to sufficiently remove organic impurities in the hollow fiber electrode green body while causing sintering of the metal particles.
As an example, the atmosphere of the second heat treatment in step a3 is one of hydrogen, argon, and a hydrogen/argon mixture; the flow rate of the atmosphere for the second heat treatment is 50-1000 mL/min, such as 50mL/min, 100mL/min, 300mL/min, 500mL/min, 700mL/min, 900mL/min, 1000mL/min, etc.; the temperature rise rate of the second heat treatment is 1-20 ℃/min, such as 1 ℃/min, 3 ℃/min, 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min and the like, the temperature of the second heat treatment is 100-1600 ℃, such as 100 ℃, 300 ℃, 600 ℃, 900 ℃, 1200 ℃, 1500 ℃, 1600 ℃ and the like, and the time of the second heat treatment is 0.5-24 h, such as 0.5h, 1h, 5h, 10h, 15h, 20h, 24h and the like.
Wherein the hydrogen/argon mixed gas comprises 10% of hydrogen and 90% of argon by volume fraction; preferably, the flow rate of the atmosphere for the second heat treatment is 100-200 mL/min, such as 100mL/min, 120mL/min, 140mL/min, 160mL/min, 180mL/min, 200mL/min, etc.; the temperature rise rate of the second heat treatment is 1-5 ℃/min, such as 1mL/min, 2mL/min, 3mL/min, 4mL/min, 5mL/min and the like, the temperature of the second heat treatment is 600-800 ℃, such as 600 ℃, 650 ℃, 700 ℃, 750 ℃, 800 ℃ and the like, and the time of the second heat treatment is 6-8 hours, such as 6 hours, 6.5 hours, 7 hours, 7.5 hours, 8 hours and the like.
In order to better understand the device, the manufacturing method and the application of the hollow fiber electrode batch heat treatment in the present invention, the present invention will be described below with reference to examples, which are only illustrative and not intended to limit the present invention in any way.
Example 1
The embodiment provides a manufacturing method of a batch heat treatment device for hollow fiber electrodes, which specifically comprises the following steps:
s1, selecting a titanium plate with the thickness of 1.0mm and the length of 500mm as a raw material, mechanically cutting and bending the titanium plate into a box body 10 with a rectangular shape, and welding and forming the titanium plate by adopting a shielded metal arc welding method;
s2, in order to prevent deformation, the periphery of the box body 10 is shaped and fixed by mechanical casting;
s3, arranging a plurality of longitudinally distributed partition layers 20 in the box body 10, and then placing the box body in a tubular furnace for roasting treatment to obtain a heat treatment device; wherein, the distance between every two adjacent partition layers 20 is 6mm, and the partition layers 20 are zigzag; the roasting treatment is to heat the titanium dioxide from 20 ℃ to 600 ℃ at the heating rate of 2 ℃/min under the air flow rate of 200ml/min, and keep the temperature for 6 hours, so as to produce a compact titanium dioxide oxide layer on the surface of the box body 10.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: the box body 10 and the partition layer 20 of cuboid form, the partition layer 20 is vertically distributed in the inside of box body 10 and sets up, and partition layer 20 is the zigzag.
The hollow fiber electrode batch heat treatment device in the embodiment is applied to batch heat treatment of Ag hollow fiber electrodes, and specifically comprises the following steps:
a1, providing a hollow fiber electrode batch heat treatment device in the present embodiment;
a2, putting the Ag hollow fiber electrode blanks with the length of 160mm pre-filled in the liner tube into the partition layer 20 of the heat treatment device in batches in sequence;
a3, placing the heat treatment device provided with the hollow fiber electrode blank in a tube furnace, carrying out first heat treatment at a temperature rising rate of 1 ℃/min to 600 ℃ for 6 hours under an atmosphere with an air flow rate of 100mL/min so as to sufficiently remove organic impurities in the blank and simultaneously cause sintering of silver particles, and then carrying out second heat treatment at a temperature rising rate of 1 ℃/min to 300 ℃ for 4 hours under an atmosphere with a hydrogen/argon mixed gas flow rate of 100mL/min so as to obtain a batch of Ag hollow fiber electrodes.
In this embodiment, 265 Ag hollow fiber electrodes are treated in a single batch, and 90% or more of the Ag hollow fiber electrodes satisfy both the conductivity and the strength.
Example 2
The present embodiment provides a method for manufacturing a hollow fiber electrode batch heat treatment apparatus, which is different from embodiment 1 in that: step S1, selecting a titanium mesh with the thickness of 1.5mm, the length of 650mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a cylindrical box body 10, and welding and forming the box body by adopting an argon arc welding method; in step S2, in order to prevent deformation, the titanium rod is used to restrain and fix the periphery of the box 10; in step S3, a plurality of partition layers 20 are disposed inside the box 10, and the baking treatment is performed for a constant temperature of 8 hours; other methods and steps are the same as those in embodiment 1, and are not described herein again.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: the box 10 and the partition layer 20 of cylindric form, the partition layer 20 is transversely distributed in the box 10 inside and is set up, and the partition layer 20 is the zigzag.
The hollow fiber electrode batch heat treatment device in the embodiment is applied to batch heat treatment of Ag hollow fiber electrodes, and the specific steps are different from those in embodiment 1 in that: the temperature rise rate of the first heat treatment in the step A3 is 2 ℃/min, the constant temperature time of the second heat treatment is 6h, and other steps and methods are the same as those in the embodiment 1 and are not repeated herein.
In the embodiment, 460 Ag hollow fiber electrodes are treated in a single batch, and more than 92% of Ag hollow fiber electrodes meet the requirements on conductivity and strength.
Example 3
The present embodiment provides a method for manufacturing a hollow fiber electrode batch heat treatment apparatus, which is different from embodiment 1 in that: step S1, selecting a titanium mesh with the thickness of 1.0mm, the length of 500mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a cylindrical box body 10, and welding and forming the box body by adopting an argon arc welding method; in step S2, in order to prevent deformation, the titanium rod is used to restrain and fix the periphery of the box 10; in the step S3, partition layers 20 are uniformly distributed in the box body 10, the distance between every two adjacent partition layers 20 is 8mm, the partition layers 20 are honeycomb-shaped, and the constant temperature time of the roasting treatment is 8 hours; other methods and steps are the same as those in embodiment 1, and are not described herein again.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: the box body 10 and the barrier layer 20 that the cylinder is form, the barrier layer 20 is honeycomb.
The hollow fiber electrode batch heat treatment device in the embodiment is applied to batch heat treatment of Ag hollow fiber electrodes, and the specific steps are different from those in embodiment 1 in that: in the step A3, the first heat treatment is to heat the mixture to 600 ℃ at a heating rate of 2 ℃/min for 6h under the atmosphere with an air flow rate of 200mL/min, and the second heat treatment is to heat the mixture to 300 ℃ at a heating rate of 1 ℃/min for 4h under the atmosphere with a hydrogen/argon mixture flow rate of 200 mL/min; other steps and methods are the same as those in embodiment 1, and are not described herein again.
In this embodiment, 340 Ag hollow fiber electrodes are treated in a single batch, and the conductivity and strength of 96% or more Ag hollow fiber electrodes satisfy the requirements.
Example 4
The present embodiment provides a method for manufacturing a hollow fiber electrode batch heat treatment apparatus, which is different from embodiment 1 in that: step S1, selecting a titanium mesh with the thickness of 1.0mm, the length of 500mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a cuboid box body 10, and welding and forming the box body by adopting an argon arc welding method; in step S2, in order to prevent deformation, mechanical molding is used to shape and fix the periphery of the box 10; in the step S3, partition layers 20 are arranged in the box body 10 in an inclined distribution, the distance between every two adjacent partition layers 20 is 10mm, the partition layers 20 are corrugated, and the constant temperature time of the roasting treatment is 8 hours; other methods and steps are the same as those in embodiment 1, and are not described herein again.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: the box body 10 and the partition layer 20 of cuboid form, partition layer 20 is the slant and distributes in the inside box body 10, and partition layer 20 is the ripple shape.
The hollow fiber electrode batch heat treatment device in the embodiment is applied to batch heat treatment of Ag hollow fiber electrodes, and the specific steps are different from those in embodiment 1 in that: in the step A2, the length of the Ag hollow fiber electrode blank is 140 mm; the temperature rise rate of the first heat treatment in the step A3 is 5 ℃/min, the temperature rise rate of the second heat treatment is 2 ℃/min, the constant temperature time is 6h, and other steps and methods are the same as those in the embodiment 1, and are not repeated herein.
In this example, 260 Ag hollow fiber electrodes were treated in a single batch, and 93% or more of the Ag hollow fiber electrodes satisfied the requirements for conductivity and strength.
Example 5
The present embodiment provides a method for manufacturing a hollow fiber electrode batch heat treatment apparatus, which is different from embodiment 1 in that: in the step S1, selecting a titanium mesh with the thickness of 1.0mm, the length of 650mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a 3/4 cylindrical box body 10, and welding and forming the box body by adopting an argon arc welding method; in step S2, in order to prevent deformation, the titanium rod is used to restrain and fix the periphery of the box 10; in the step S3, longitudinally distributed partition layers 20 are arranged inside the box body 10, the distance between every two adjacent partition layers 20 is 8mm, the partition layers 20 are corrugated, and the constant temperature time of the roasting treatment is 8 hours; other methods and steps are the same as those in embodiment 1, and are not described herein again.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: 3/4 cylindrical case 10 and a partition layer 20, wherein the partition layer 20 is longitudinally distributed inside the case 10, and the partition layer 20 is corrugated. As shown in fig. 1 and 2.
The hollow fiber electrode batch heat treatment device in the embodiment is applied to batch heat treatment of Ag hollow fiber electrodes, and the specific steps are different from those in embodiment 1 in that: the temperature rise rate of the first heat treatment in the step A3 is 2 ℃/min, the temperature rise rate of the second heat treatment is 350 ℃, and other steps and methods are the same as those in the embodiment 1, and are not repeated.
In this embodiment, 450 Ag hollow fiber electrodes treated in a single batch, and more than 95% of the Ag hollow fiber electrodes satisfy both the conductivity and the strength.
Example 6
The embodiment provides a manufacturing method of a batch heat treatment device for hollow fiber electrodes, which specifically comprises the following steps:
s1, selecting a titanium plate with the thickness of 0.5mm and the length of 600mm as a raw material, mechanically cutting and bending the titanium plate into a 2/3 cylindrical box body 10, and welding and forming the box body by adopting a laser welding method;
s2, in order to prevent deformation, the periphery of the box body 10 is restrained and fixed by a titanium rod;
s3, arranging a plurality of transversely distributed partition layers 20 in the box body 10, and then placing the box body in a tubular furnace for roasting treatment to obtain a heat treatment device; wherein, the distance between every two adjacent partition layers 20 is 8mm, and the partition layers 20 are corrugated; the roasting treatment is to heat the titanium dioxide from 20 ℃ to 600 ℃ at the heating rate of 2 ℃/min under the air flow rate of 200ml/min, and keep the temperature for 8 hours, so as to produce a compact titanium dioxide oxide layer on the surface of the box body 10.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: 2/3 cylindrical case 10 and a partition layer 20, wherein the partition layer 20 is distributed transversely inside the case 10, and the partition layer 20 is corrugated.
The batch heat treatment device for the hollow fiber electrode in the embodiment is applied to batch heat treatment of the Ni hollow fiber electrode, and specifically comprises the following steps:
a1, providing a hollow fiber electrode batch heat treatment device in the present embodiment;
a2, putting the Ni hollow fiber electrode blanks with the length of 120mm pre-filled in the liner tube into the partition layer 20 of the heat treatment device in batches in sequence;
a3, placing the heat treatment device with the hollow fiber electrode blank in a tube furnace, carrying out first heat treatment at a constant temperature of 6h from a heating rate of 2 ℃/min to 600 ℃ in an atmosphere with an air flow rate of 200mL/min so as to sufficiently remove organic impurities in the blank and simultaneously cause sintering of Ni particles, and then carrying out second heat treatment at a constant temperature of 6h from a heating rate of 1 ℃/min to 600 ℃ in an atmosphere with a hydrogen/argon mixed gas flow rate of 200mL/min so as to obtain a batch of Ni hollow fiber electrodes.
In this example, 420 Ni hollow fiber electrodes were processed in a single batch, and the conductivity and strength of 91% or more Ni hollow fiber electrodes were satisfactory.
Example 7
The present embodiment provides a method for manufacturing a hollow fiber electrode batch heat treatment apparatus, which is different from embodiment 6 in that: in step S1, selecting a titanium mesh with the thickness of 1.5mm, the length of 650mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a cylindrical box body 10, and welding and forming the box body by adopting a laser welding method; in step S3, honeycomb-shaped partition layers 20 are uniformly distributed inside the box body 10, and the distance between every two adjacent partition layers 20 is 6 mm; other methods and steps are the same as those in embodiment 6, and are not described herein again.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: the box 10 and the partition layer 20 of cylinder form, the partition layer 20 evenly distributes at the box 10, and the partition layer 20 is honeycomb.
The hollow fiber electrode batch heat treatment device in this embodiment is applied to batch heat treatment of Ni hollow fiber electrodes, and the specific steps are different from those in embodiment 6 in that: the length of the Ni hollow fiber electrode blank in the step A2 is 100 mm; in the step A3, the heating rate of the first heat treatment is 5 ℃/min, and the heating rate of the second heat treatment is 2 ℃/min; other steps and methods are the same as those in embodiment 6, and are not described herein again.
In this example, 690 single batch-processed Ni hollow fiber electrodes satisfied both the conductivity and strength of 97% or more Ni hollow fiber electrodes.
Example 8
The present embodiment provides a method for manufacturing a batch heat treatment apparatus for hollow fiber electrodes, which is different from embodiment 6 in that: step S1, selecting a titanium mesh with the thickness of 1.0mm, the length of 600mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a cylindrical box body 10, and welding and forming the box body by adopting an argon arc welding method; in step S3, honeycomb-shaped partition layers 20 are uniformly distributed inside the box body 10, and the distance between every two adjacent partition layers 20 is 6 mm; other methods and steps are the same as those in embodiment 6, and are not described herein again.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: the box body 10 and the partition layer 20 that the box body 10 is the cylindricality, and the partition layer 20 is evenly distributed at the box body 10, and the partition layer 20 is honeycomb.
The hollow fiber electrode batch heat treatment device in this embodiment is applied to batch heat treatment of Ni hollow fiber electrodes, and the specific steps are different from those in embodiment 6 in that: in the step A2, the length of the Ni hollow fiber electrode blank is 180 mm; in the step A3, the heating rate of the first heat treatment is 5 ℃/min, and the heating rate of the second heat treatment is 2 ℃/min; other steps and methods are the same as those in embodiment 6, and are not described herein again.
In this example, 320 Ni hollow fiber electrodes were processed in a single batch, and the conductivity and strength of 93% or more Ni hollow fiber electrodes satisfied the requirements.
Example 9
The present embodiment provides a method for manufacturing a batch heat treatment apparatus for hollow fiber electrodes, which is different from embodiment 6 in that: in step S1, a titanium mesh with a thickness of 0.5mm, a length of 500mm and a pore diameter of 2 × 4mm is selected as a raw material, mechanically cut and bent into a rectangular box 10, and welded and formed by an argon arc welding method; in step S2, in order to prevent deformation, mechanical casting is used for fixing and shaping; in step S3, the partition layers 20 are longitudinally distributed in the box body 10, and the distance between every two adjacent partition layers 20 is 6 mm; other methods and steps are the same as those in embodiment 6, and are not described herein again.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: the box body 10 is rectangular parallelepiped, and the blocking layer 20, the blocking layer 20 is distributed in the box body 10 longitudinally, and the blocking layer 20 is zigzag.
The hollow fiber electrode batch heat treatment device in this embodiment is applied to batch heat treatment of Ni hollow fiber electrodes, and the specific steps are different from those in embodiment 6 in that: the length of the Ni hollow fiber electrode blank in the step A2 is 160 mm; in the step A3, the air flow rate of the first heat treatment is 100mL/min, the flow rate of the hydrogen/argon mixed gas of the second heat treatment is 100mL/min, and the temperature rise rate is 2 ℃/min; other steps and methods are the same as those in embodiment 6, and are not described herein again.
In this example, 255 Ni hollow fiber electrodes were processed in a single batch, and the conductivity and strength of 93% or more Ni hollow fiber electrodes satisfied the requirements.
Example 10
The present embodiment provides a method for manufacturing a batch heat treatment apparatus for hollow fiber electrodes, which is different from embodiment 6 in that: in the step S1, selecting a titanium mesh with the thickness of 1.0mm, the length of 600mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a 3/4 cylindrical box body 10, and welding and forming the box body by adopting an argon arc welding method; in step S3, zigzag partition layers 20 are obliquely distributed inside the box body 10, and the distance between every two adjacent partition layers 20 is 6 mm; other methods and steps are the same as those in embodiment 6, and are not described herein again.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: 3/4 a cylindrical case 10 and a partition layer 20, wherein the partition layer 20 is distributed obliquely in the case 10, and the partition layer 20 is zigzag.
The hollow fiber electrode batch heat treatment device in this embodiment is applied to batch heat treatment of Ni hollow fiber electrodes, and the specific steps are different from those in embodiment 6 in that: in the step A3, the temperature rise rate of the first heat treatment is 5 ℃/min, the flow rate of the hydrogen/argon mixed gas of the second heat treatment is 100mL/min, the temperature rise rate is 2 ℃/min to 600 ℃, and the temperature is kept constant for 4 h; other steps and methods are the same as those in embodiment 6, and are not described herein again.
In this example, 500 Ni hollow fiber electrodes were processed in a single batch, and the conductivity and strength of 90% or more of the Ni hollow fiber electrodes satisfied the requirements.
Example 11
The embodiment provides a manufacturing method of a batch heat treatment device for hollow fiber electrodes, which specifically comprises the following steps:
s1, selecting a titanium plate with the thickness of 1.0mm and the length of 650mm as a raw material, mechanically cutting and bending the titanium plate into a cylindrical box body 10, and welding and forming the box body by adopting a laser welding method;
s2, in order to prevent deformation, the periphery of the box body 10 is restrained and fixed by titanium bars;
s3, arranging a plurality of longitudinally distributed partition layers 20 in the box body 10, and then placing the box body in a tubular furnace for roasting treatment to obtain a heat treatment device; wherein, the distance between every two adjacent partition layers 20 is 10mm, and the partition layers 20 are corrugated; the roasting treatment is to heat the titanium dioxide from 20 ℃ to 600 ℃ at the heating rate of 2 ℃/min under the air flow rate of 200ml/min, and keep the temperature for 8 hours, so as to produce a compact titanium dioxide oxide layer on the surface of the box body 10.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: the box 10 and the partition layer 20 of cylinder form, partition layer 20 is vertically distributed in the inside of box 10, and partition layer 20 is the wave form.
The hollow fiber electrode batch heat treatment device in the embodiment is applied to batch heat treatment of the Cu hollow fiber electrode, and specifically comprises the following steps:
a1, providing a hollow fiber electrode batch heat treatment device in the present embodiment;
a2, sequentially putting the Cu hollow fiber electrode blanks with the length of 160mm pre-filled in the liner tube into the partition layer 20 of the heat treatment device in batches;
a3, placing the heat treatment device provided with the hollow fiber electrode blank in a tube furnace, carrying out first heat treatment at a constant temperature of 4 hours from a heating rate of 5 ℃/min to 550 ℃ in an atmosphere with an air flow rate of 200mL/min so as to sufficiently remove organic impurities in the blank and simultaneously cause sintering of Cu particles, and then carrying out second heat treatment at a constant temperature of 6 hours from a heating rate of 1 ℃/min to 600 ℃ in an atmosphere with a hydrogen/argon mixed gas flow rate of 200mL/min so as to obtain a batch of Cu hollow fiber electrodes.
In this example, the conductivity and strength of each of the single batch-processed Cu hollow fiber electrodes were satisfactory for 450 or more Cu hollow fiber electrodes and 90% or more of the Cu hollow fiber electrodes.
Example 12
The present embodiment provides a method for manufacturing a batch heat treatment apparatus for hollow fiber electrodes, which is different from embodiment 11 in that: in the step S1, selecting a titanium mesh with the thickness of 1.0mm, the length of 650mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a 2/3 cylindrical box body 10, and welding and forming the box body by adopting an argon arc welding method; in step S3, honeycomb partition layers 20 with the space of 8mm are uniformly distributed in the box body 10; other methods and steps are the same as those in embodiment 11, and are not described herein again.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: 2/3 cylindrical case 10 and a partition layer 20, wherein the partition layer 20 is uniformly distributed in the case 10, and the partition layer 20 is honeycomb-shaped.
The hollow fiber electrode batch heat treatment device in the present embodiment is applied to the batch heat treatment of the Cu hollow fiber electrode, and the specific steps are different from those in embodiment 11 in that: the length of the Cu hollow fiber electrode blank in the step A2 is 140 mm; in the step A3, the heating rate of the first heat treatment is 2 ℃/min, and the temperature is kept for 6 h; other steps and methods are the same as those in embodiment 11, and are not described herein again.
In this example, the conductivity and strength of 340 Cu hollow fiber electrodes treated in a single batch satisfied the requirements of 97% or more of the Cu hollow fiber electrodes.
Example 13
The present embodiment provides a method for manufacturing a hollow fiber electrode batch heat treatment apparatus, which is different from embodiment 11 in that: in step S1, a titanium mesh having a thickness of 1.0mm, a length of 550mm and a pore size of 2 × 4mm is selected as a raw material, and is mechanically cut and bent into a rectangular box 10, and welded and formed by an argon arc welding method; in step S2, in order to prevent deformation, mechanical coining is used for shaping and fixing; in step S3, honeycomb partition layers 20 with the space of 8mm are uniformly distributed in the box body 10; other methods and steps are the same as those in embodiment 11, and are not described herein again.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: the box body 10 and the partition layer 20 of cuboid form, partition layer 20 is evenly distributed in box body 10, and partition layer 20 is honeycomb.
The hollow fiber electrode batch heat treatment device in the embodiment is applied to the batch heat treatment of the Cu hollow fiber electrode, and the specific steps are different from those in embodiment 11 in that: in the step A2, the length of the Cu hollow fiber electrode blank is 120 mm; in the step A3, the temperature of the first heat treatment is kept constant for 6h at the temperature rising rate of 2 ℃/min to 600 ℃ in the atmosphere with the air flow rate of 200mL/min, and the temperature of the second heat treatment is kept constant for 8 h; other steps and methods are the same as those in embodiment 11, and are not described herein again.
In this example, 300 Cu hollow fiber electrodes were treated in a single batch, and the conductivity and strength of 98% or more of the Cu hollow fiber electrodes satisfied the requirements.
Example 14
The present embodiment provides a method for manufacturing a hollow fiber electrode batch heat treatment apparatus, which is different from embodiment 11 in that: in step S1, selecting a titanium mesh with the thickness of 1.0mm, the length of 500mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a cylindrical box body 10, and welding and forming the titanium mesh by adopting an argon arc welding method; in step S3, zigzag partition layers 20 with a pitch of 6mm are transversely and uniformly distributed in the box body 10; other methods and steps are the same as those in embodiment 11, and are not described herein again.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: the box 10 and the partition layer 20 of cylinder form, the horizontal evenly distributed of partition layer 20 in box 10, and partition layer 20 is the zigzag.
The hollow fiber electrode batch heat treatment device in the present embodiment is applied to the batch heat treatment of the Cu hollow fiber electrode, and the specific steps are different from those in embodiment 11 in that: the length of the Cu hollow fiber electrode blank in the step A2 is 180 mm; in the step A3, the first heat treatment is carried out at the temperature rising rate of 2 ℃/min to 600 ℃ for 6h under the atmosphere with the air flow rate of 200 mL/min; other steps and methods are the same as those in embodiment 11, and are not described herein again.
In this example, 275 single-batch-processed Cu hollow fiber electrodes were satisfied in both conductivity and strength of 90% or more of the Cu hollow fiber electrodes.
Example 15
The present embodiment provides a method for manufacturing a hollow fiber electrode batch heat treatment apparatus, which is different from embodiment 11 in that: in the step S1, selecting a titanium mesh with the thickness of 1.0mm, the length of 600mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a 3/4 cylindrical box body 10, and welding and forming the box body by adopting an argon arc welding method; in step S3, honeycomb partition layers 20 with a pitch of 8mm are uniformly distributed in the box body 10, and the pitch between every two adjacent partition layers 20 is 6 mm; other methods and steps are the same as those in embodiment 11, and are not described herein again.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: 3/4 cylindrical case 10 and a partition layer 20, wherein the partition layer 20 is uniformly distributed in the case 10, and the partition layer 20 is honeycomb-shaped.
The hollow fiber electrode batch heat treatment device in the present embodiment is applied to the batch heat treatment of the Cu hollow fiber electrode, and the specific steps are different from those in embodiment 11 in that: the length of the Cu hollow fiber electrode blank in the step A2 is 140 mm; the first heat treatment in the step A3 is constant in temperature for 6 hours; other steps and methods are the same as those in embodiment 11, and are not described herein again.
In this example, 365 Cu hollow fiber electrodes were processed in a single batch, and the conductivity and strength of 96% or more of the Cu hollow fiber electrodes satisfied the requirements.
Example 16
The embodiment provides a manufacturing method of a batch heat treatment device for hollow fiber electrodes, which specifically comprises the following steps:
s1, selecting a titanium mesh with the thickness of 1.0mm, the length of 600mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a 3/4 cylindrical box body 10, and welding and forming the box body by adopting an argon arc welding method;
s2, in order to prevent deformation, the periphery of the box body 10 is restrained and fixed by titanium bars;
s3, arranging a plurality of partition layers 20 which are uniformly distributed in the box body 10, and then placing the box body in a tubular furnace for roasting treatment to obtain a heat treatment device; wherein, the distance between every two adjacent partition layers 20 is 8mm, and the partition layers 20 are honeycomb-shaped; the roasting treatment is to heat the titanium dioxide from 20 ℃ to 600 ℃ at the heating rate of 2 ℃/min under the air flow rate of 200ml/min, and keep the temperature for 8 hours, so as to produce a compact titanium dioxide oxide layer on the surface of the box body 10.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: 3/4 cylindrical case 10 and a partition layer 20, wherein the partition layer 20 is uniformly distributed in the case 10, and the partition layer 20 is honeycomb-shaped.
The hollow fiber electrode batch heat treatment device in the embodiment is applied to batch heat treatment of Fe hollow fiber electrodes, and specifically comprises the following steps:
a1, providing a hollow fiber electrode batch heat treatment device in the present embodiment;
a2, putting the Fe hollow fiber electrode blanks with the length of 140mm pre-filled in the liner tube into the partition layer 20 of the heat treatment device in batches in sequence;
a3, placing the heat treatment device provided with the hollow fiber electrode blank in a tube furnace, carrying out first heat treatment at a constant temperature of 6 hours from a heating rate of 5 ℃/min to 600 ℃ in an atmosphere with an air flow rate of 200mL/min so as to sufficiently remove organic impurities in the blank and simultaneously cause sintering of Fe particles, and then carrying out second heat treatment at a constant temperature of 6 hours from a heating rate of 2 ℃/min to 600 ℃ in an atmosphere with a hydrogen/argon mixed gas flow rate of 200mL/min so as to obtain a batch of Fe hollow fiber electrodes.
In this example, 365 Fe hollow fiber electrodes treated in a single batch satisfied the conductivity and strength of 98% or more Fe hollow fiber electrodes.
Example 17
The present example provides a method for manufacturing a hollow fiber electrode batch heat treatment apparatus, which is different from example 16 in that: in step S1, a titanium plate with a thickness of 1.0mm and a length of 550mm is selected as a raw material, and is mechanically cut and bent into a rectangular box 10, and welded and formed by an argon arc welding method; in step S2, in order to prevent deformation, mechanical casting is used for fixing and shaping; in step S3, transversely distributing corrugated partition layers 20 with the space of 8mm in the box body 10; the other methods and steps are the same as those in example 16, and are not described in detail herein.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: the box body 10 and the partition layer 20 of cuboid form, the partition layer 20 is transversely distributed in the box body 10, and the partition layer 20 is corrugated.
The hollow fiber electrode batch heat treatment device in this embodiment is applied to batch heat treatment of Fe hollow fiber electrodes, and the specific steps are different from those in embodiment 16 in that: in the step A2, the length of the Fe hollow fiber electrode blank is 120 mm; in the step A3, the heating rate of the first heat treatment is 2 ℃/min, and the heating rate of the second heat treatment is 1 ℃/min; the other steps and methods are the same as those in example 16, and are not described in detail herein.
In this example, 310 Fe hollow fiber electrodes were treated in a single batch, and the conductivity and strength of the Fe hollow fiber electrodes of 92% or more satisfied the requirements.
Example 18
The present example provides a method for manufacturing a hollow fiber electrode batch heat treatment apparatus, which is different from example 16 in that: in step S1, selecting a titanium mesh with the thickness of 1.0mm, the length of 500mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a cylindrical box body 10, and welding and forming the titanium mesh by adopting an argon arc welding method; in step S3, the zigzag partition layers 20 with a pitch of 8mm are obliquely distributed inside the box body 10; the other methods and steps are the same as those in example 16, and are not described in detail herein.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: the cylindrical box body 10 and the partition layer 20, the partition layer 20 distributes in the box body 10 slant, and the partition layer 20 is the zigzag.
The hollow fiber electrode batch heat treatment device in this embodiment is applied to batch heat treatment of Fe hollow fiber electrodes, and the specific steps are different from those in embodiment 16 in that: the length of the Fe hollow fiber electrode blank in the step A2 is 160 mm; in the step A3, the temperature of the first heat treatment is kept constant for 4 hours, and the temperature of the second heat treatment is increased to 800 ℃; the other steps and methods are the same as those in example 16, and are not described in detail herein.
In this example, the single batch processed Fe hollow fiber electrodes 335 had the conductivity and strength of the Fe hollow fiber electrodes of 94% or more that satisfied the requirements.
Example 19
The present example provides a method for manufacturing a hollow fiber electrode batch heat treatment apparatus, which is different from example 16 in that: in the step S1, selecting a titanium mesh with the thickness of 1.5mm, the length of 650mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a 2/3 cylindrical box body 10, and welding and forming the box body by adopting an argon arc welding method; in step S3, corrugated partition layers 20 with the space of 8mm are longitudinally distributed in the box body 10, and the roasting treatment is carried out for 10 hours at constant temperature; the other methods and steps are the same as those in example 16, and are not described in detail herein.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: 2/3 cylindrical case 10 and a partition layer 20, the partition layer 20 is distributed longitudinally in the case 10, and the partition layer 20 is corrugated.
The hollow fiber electrode batch heat treatment device in this embodiment is applied to batch heat treatment of Fe hollow fiber electrodes, and the specific steps are different from those in embodiment 16 in that: in the step A2, the length of the Fe hollow fiber electrode blank is 100 mm; the heating rate of the first heat treatment in the step A3 is 2 ℃/min; the other steps and methods are the same as those in example 16, and are not described in detail herein.
In this example, the single batch treatment of 520 Fe hollow fiber electrodes satisfied both the conductivity and strength of 96% or more Fe hollow fiber electrodes.
Example 20
The present example provides a method for manufacturing a hollow fiber electrode batch heat treatment apparatus, which is different from example 16 in that: in the step S1, selecting a titanium mesh with the thickness of 0.5mm, the length of 600mm and the aperture of 2 multiplied by 4mm as a raw material, mechanically cutting and bending the titanium mesh into a semi-cylindrical box body 10, and welding and forming the titanium mesh by adopting an argon arc welding method; in step S3, uniformly distributing honeycomb partition layers 20 with the space of 6mm in the box body 10; the other methods and steps are the same as those in example 16, and are not described in detail herein.
The present embodiment also provides a batch heat treatment apparatus for hollow fiber electrodes, including: the semi-cylindrical box body 10 and the partition layer 20, the partition layer 20 is evenly distributed in the box body 10, and the partition layer 20 is honeycomb-shaped.
The hollow fiber electrode batch heat treatment device in this embodiment is applied to batch heat treatment of Fe hollow fiber electrodes, and the specific steps are different from those in embodiment 16 in that: in the step A2, the length of the Fe hollow fiber electrode blank is 120 mm; in the step A3, the heating rate of the first heat treatment is 2 ℃/min, the temperature of the second heat treatment is raised to 800 ℃, and the temperature is kept for 8 hours; the other steps and methods are the same as those in example 16, and are not described in detail herein.
In this example, 380 single batch processed Fe hollow fiber electrodes satisfied both the conductivity and strength of 94% or more Fe hollow fiber electrodes.
In summary, the invention provides a device which is simple in design, simple and convenient to operate, and capable of being used for batch heat treatment of hollow fiber electrodes quickly and efficiently, wherein metal titanium or tungsten with high melting point, low mass density, strong bending ductility, strong corrosion resistance and strong oxidation resistance is used as a raw material of the device, the device is ensured to be stable under high-temperature oxidation or reduction conditions by mechanical cutting, bending, welding, fixing and forming, and partition layers with different structural forms are arranged in the device, so that the device is free from pollution to a target material, the uniformity of a thermal radiation field and a gas flow field in the heat treatment process is controlled, the uniformity and repeatability of heat treatment of the target material are ensured, the target material can be subjected to heat treatment quickly and massively, and the production efficiency is greatly improved; the batch heat treatment device can be used for batch treatment of hundreds to thousands of hollow fiber electrode samples once, effectively simplifies the batch production process of the hollow fiber electrodes, improves the production efficiency, forms an efficient, stable and low-cost preparation process amplification scheme, promotes large-scale production and application of the hollow fiber electrodes, can be widely applied to the production process of various hollow fiber electrodes, and has extremely high application prospects. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Those skilled in the art can modify or change the above-described embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (10)

1. The manufacturing method of the hollow fiber electrode batch heat treatment device is characterized by comprising the following steps of:
s1, mechanically cutting and bending the raw materials into a box body, and welding and forming;
s2, fixing the box body at the periphery;
and S3, arranging a plurality of partition layers in the box body, and then placing the box body in a tubular furnace for roasting treatment to obtain the heat treatment device.
2. The manufacturing method of the hollow fiber electrode batch heat treatment device according to claim 1, characterized in that: step S1 includes one or a combination of the following conditions:
the raw material is one or a combination of a titanium plate, a titanium mesh, a tungsten plate and a tungsten mesh;
the thickness of the raw material is 0.1-2.5 mm;
the box body is in one shape of a cuboid, a cylinder, a semi-cylinder, an 3/4 cylinder and a 2/3 cylinder;
the welding method is one or combination of shielded metal arc welding, argon arc welding and laser welding.
3. The manufacturing method of the hollow fiber electrode batch heat treatment device according to claim 1, characterized in that: the fixing mode in the step S2 is one of titanium rod constraint fixing, tungsten rod constraint fixing, and mechanical cast-pressing fixing.
4. The manufacturing method of the hollow fiber electrode batch heat treatment device according to claim 1, characterized in that: step S3 includes one or a combination of the following conditions:
the distance between every two adjacent partition layers is 5-10 mm;
the partition layer is in one or a combination of a sawtooth shape, a corrugated shape and a honeycomb shape;
the setting direction of the partition layer is one or more of a transverse partition, a longitudinal partition and an oblique partition.
5. The manufacturing method of the hollow fiber electrode batch heat treatment device according to claim 1, characterized in that: step S3 includes one or a combination of the following conditions:
the roasting atmosphere is oxygen or air atmosphere, and the roasting atmosphere flow rate is 100-300 mL/min;
the heating rate of the roasting is 1-20 ℃/min, the roasting temperature is 400-1000 ℃, and the roasting time is 4-12 h.
6. A hollow fiber electrode batch heat treatment apparatus manufactured by the manufacturing method of the hollow fiber electrode batch heat treatment apparatus according to any one of claims 1 to 5, characterized in that: the heat treatment apparatus includes:
the box body is in a cuboid, cylinder, semi-cylinder, 3/4 cylinder or 2/3 cylinder shape, and an anti-deformation structure is fixed along the length direction of the box body;
the partition layer, it is provided with a plurality ofly to block the layer, and is a plurality of block the even setting in of layer inside the box, just block the layer and be zigzag, corrugated or honeycombed.
7. The application of the hollow fiber electrode batch heat treatment device is characterized in that the hollow fiber electrode batch heat treatment device is applied to batch heat treatment of the hollow fiber electrode, and specifically comprises the following steps:
a1, providing the hollow fiber electrode batch heat treatment device of claim 6;
a2, sequentially placing the hollow fiber electrode green blanks which are pre-filled in the liner tube into the partition layer of the heat treatment device in batches;
a3, placing the heat treatment device provided with the hollow fiber electrode blank in a tube furnace, carrying out first heat treatment in an air atmosphere, and then carrying out second heat treatment in a gas atmosphere to obtain a batch of hollow fiber electrodes.
8. Use of a hollow fiber electrode batch heat treatment apparatus according to claim 7, characterized in that: the hollow fiber electrode blank in the step A2 is made of one of silver, copper, iron, cobalt, nickel, titanium, bismuth oxide and tin oxide;
the length of the hollow fiber electrode blank is 100-200 mm.
9. Use of a hollow fiber electrode batch heat treatment apparatus according to claim 7, characterized in that: the atmosphere of the first heat treatment in the step A3 is air; the flow rate of the atmosphere for the first heat treatment is 100-200 mL/min; the temperature rise rate of the first heat treatment is 1-5 ℃/min; the temperature of the first heat treatment is 550-600 ℃; the time of the first heat treatment is 4-6 h.
10. Use of a hollow fiber electrode batch heat treatment apparatus according to claim 7, characterized in that: the atmosphere of the second heat treatment in the step A3 is one of hydrogen, argon and hydrogen/argon mixed gas; the flow rate of the atmosphere for the second heat treatment is 50-1000 mL/min; the temperature rise rate of the second heat treatment is 1-20 ℃/min, the temperature of the second heat treatment is 100-1600 ℃, and the time of the second heat treatment is 0.5-24 h.
CN202210494162.XA 2022-05-05 2022-05-05 Hollow fiber electrode batch heat treatment device, manufacturing method and application Active CN114932376B (en)

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